CN110658360B - Method and device for preparing superfine atomic force microscope metal probe - Google Patents
Method and device for preparing superfine atomic force microscope metal probe Download PDFInfo
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- CN110658360B CN110658360B CN201910870484.8A CN201910870484A CN110658360B CN 110658360 B CN110658360 B CN 110658360B CN 201910870484 A CN201910870484 A CN 201910870484A CN 110658360 B CN110658360 B CN 110658360B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
- G01Q60/40—Conductive probes
Abstract
The invention discloses a method and a device for preparing a superfine atomic force microscope metal probe. Respectively preparing a homogeneous metal cut end and a metal needle tip, wherein the metal cut end is arranged at the fixed end of the electro-mechanical sample rod, the metal needle tip is loaded at the movable end, and the two ends are oppositely arranged without contact. In a transmission electron microscope, aligning and approaching a metal needle tip to a fracture sample by piezoelectric ceramic drive; and applying constant bias voltage to two ends of the critical contact point, and realizing the preparation of the superfine atomic force microscope metal probe by utilizing the electro atomic migration effect. The preparation method of the atomic force microscope metal probe has the advantages of high success rate, controllable growth direction and length of a finished product, small tip diameter of less than 5nm, and good stability and conductivity.
Description
Technical Field
The invention relates to the technical field of micro-nano manufacturing, in particular to an in-situ preparation method and device of a single metal probe of a controllable superfine atomic force microscope.
Background
An Atomic Force Microscope (AFM) is a micrometer-scale precision mechanical measuring instrument invented by Binning et al in 1986, and an AFM probe is one of key components for realizing precision measurement and mainly comprises a substrate, a micro-cantilever and a needle tip at the free end of the cantilever, wherein the micro-cantilever is extremely sensitive to weak Force. When the sample is scanned, the probe and the surface of the sample are close to each other, and the interaction force between the probe tip atoms and the sample surface atoms is rapidly increased along with the reduction of the distance between the probe tip atoms and the sample surface atoms, so that the cantilever beam generates tiny displacement. This small displacement is detected and used as feedback to keep the force constant to obtain the change in position of the microcantilever corresponding to the points scanned, and finally to obtain an image of the surface topography of the sample. The atomic force microscope can analyze the surface appearance of a sample on an atomic scale, can also carry out atomic etching processing on the surface of the sample, and plays a great role in the fields of physics, chemistry, materials science, life science, microelectronic technology and the like.
As a core component of atomic force microscopy, the physicochemical properties and geometry of the AFM probe tip will significantly affect the final imaging quality.
The conventional AFM probe mainly comprises silicon, silicon nitride, carbon nanotube and other materials. Among them, the micro-cantilever-tip integrated structure formed by processing silicon or silicon nitride by etching, sputtering deposition and other techniques is the most common. However, silicon and silicon nitride materials have low reflectivity in the visible and near infrared, and usually a metal layer needs to be plated on the cantilever to improve the reflectivity, so that the radius of curvature of the tip is large, and the situation of the bottom of the atomic-scale structure is difficult to directly observe. Moreover, such conventional AFM probes are generally pyramid-shaped or cone-shaped, have large diameters, are brittle, and are easily broken. However, the carbon nanotube has the advantages of small diameter, good flexibility and the like, but the angle and the length-diameter ratio of the probe cannot be controlled by the current main preparation method (including a growth method, a pickup method, an electrophoresis method, a mechanical manipulation method and the like) of the carbon nanotube AFM probe, so that a single high-quality probe is difficult to obtain. Therefore, a new high-quality AFM probe preparation method is needed.
Disclosure of Invention
In order to solve the problems existing in the background technology, the invention aims to provide an in-situ preparation method and a device of a controllable superfine atomic force microscope metal probe, wherein the growth position and the state can be directly observed during preparation, the preparation method can be used for preparing the superfine atomic force microscope metal probe with controllable length and growth direction and the diameter of the tip of less than 5nm with higher success rate, and the technical problem that the growth position and the state cannot be directly observed and controlled during preparation in the prior art is solved.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a superfine atomic force microscope metal probe comprises the following steps:
the method comprises an electro-mechanical single-inclination sample rod, wherein the electro-mechanical single-inclination sample rod comprises two parts, namely a movable end and a fixed end, the movable end and the fixed end are oppositely arranged and are not contacted, and a metal needle point and a metal cut-off end are respectively loaded on the movable end and the fixed end; then the following steps are adopted for processing:
1) preparing a metal fracture end by adopting a physical shearing method, specifically, flattening the tail end of a metal wire with the diameter of about 0.25mm, and then shearing the metal wire to be used as the metal fracture end, wherein the metal fracture end is fixed at a fixed end;
2) carrying out electrochemical corrosion treatment on the tail end of the metal wire to prepare a metal needle point with a sharp tail end, wherein the diameter of the metal needle point is in the range of 50 nanometers to 200 nanometers, the root of the metal needle point is fixed at the movable end, and the tip of the metal needle point faces the end of the metal fracture;
3) placing the electro-mechanical single-inclined sample rod into a transmission electron microscope sample cavity, and driving the metal needle tip to be horizontally aligned and close to the metal fracture end in the transmission electron microscope sample cavity by utilizing piezoelectric ceramics;
4) preparing an atomic force microscope metal probe: applying a constant bias voltage of 600 plus 1000mV at two ends of the electricity-mechanics single-inclination sample rod under a critical contact point, wherein the voltage is determined according to a metal system, moving the movable end of the electricity-mechanics single-inclination sample rod under the observation of a transmission electron microscope, moving the movable end of the metal needle point to enable the gap between the metal needle point and the metal cut end to be approximate to about 2nm, and connecting the two close parts under the action of electromigration to form a single-crystal metal nanowire; then moving the movable end of the metal needle tip at a constant speed in the direction away from the fixed end to separate the two ends to obtain a single superfine atomic force microscope metal probe with a certain length;
5) and (4) repeating the step 4), wherein the atomic force microscope metal probe stably grows along the axial direction, continuously grows and extends vertically, and is regulated and controlled for multiple times to obtain the final atomic force microscope metal probe with ideal length and appearance, small diameter and large length-diameter ratio.
The two ends are enabled to grow close to each other continuously, and the atomic force microscope metal probe grows and extends vertically continuously to obtain the final atomic force microscope metal probe with small diameter and large length-diameter ratio.
The obtained metal probe of the atomic force microscope has the diameter less than 5nm and controllable length, and the length is determined by voltage, moving speed and contact times.
The growth direction of the atomic force microscope metal probe is controlled by adjusting the polarity of a power supply connected with the metal tip and the metal cut-off end.
The metal tip 1 and the metal cut-off end 2 are respectively connected with the negative electrode and the positive electrode of the power supply 3, and the atomic force microscope metal probe vertically grows from the surface of the metal tip 1 to the direction of the metal cut-off end 2.
The metal tip 1 and the metal cut-off end 2 are respectively connected with the anode and the cathode of a power supply 3, and the atomic force microscope metal probe vertically grows from the surface of the metal cut-off end 2 to the direction of the metal tip 1.
The metal material of the metal needle tip and the metal fracture end is a homogeneous metal material, including but not limited to tungsten, gold or molybdenum and other metal materials.
Secondly, a controllable atomic force microscope metal probe preparation device:
the device comprises an electrochemical corrosion system, a transmission electron microscope and an electro-mechanical single-inclination sample rod, wherein the transmission electron microscope is used for recording and observing the growth preparation condition of a probe between a metal needle point and a metal fracture end of the electro-mechanical single-inclination sample rod and the relative position and movement condition of the metal needle point and the metal fracture end; the electrochemical corrosion system is used for processing the metal wire to obtain the preparation of the metal needle tip.
The electro-mechanical single-inclination sample rod comprises two parts, namely a movable end and a fixed end, wherein the movable end and the fixed end are oppositely arranged and are not contacted, and a metal needle point and a metal cut-off end are respectively fixed on the movable end and the fixed end; the metal needle tip and the metal fracture end are respectively connected with the anode and the cathode of a power supply. In the experiment, the movable end can be driven to realize accurate control and voltage application in the vertical, left-right, front-back and three-dimensional directions.
Compared with the prior art, the invention has the advantages that:
1. the growth direction and the geometric dimension of the probe can be observed and controlled in situ;
2. the growth direction of the crystal can be controlled and the superfine probe with extremely high length-diameter ratio can be obtained;
3. the preparation success rate is high, and the probe is not easy to fall off or wear;
4. the application range is wide, and the method is suitable for various metal materials such as gold, tungsten, molybdenum and the like;
5. the metal probe is directly grown on the metal wire, and the stability and the conductivity are good.
Drawings
FIG. 1 is a schematic view of a production system of the present invention;
fig. 2 is a physical diagram of the metal tip 1 and the metal cut end 2;
FIG. 3 is a transmission electron microscope set diagram of an in-situ preparation process of the electron probe in the case that the metal tip 1 and the metal open end 2 are respectively connected with the cathode and the anode of the power supply 3 in the embodiment 1;
wherein (a) is transmission electron microscope picture of the metal needle point and the metal cut end before the preparation
(b) (c) transmission electron microscope picture of atomic force microscope metal probe appearance and growth process after voltage is applied
(d) The prepared atomic force microscope metal probe picture is obtained;
FIG. 4 is a transmission electron microscope set diagram of an in-situ preparation process of the electron probe in the case of the embodiment 2 in which the metal tip 1 and the metal open end 2 are respectively connected to the positive electrode and the negative electrode of the power supply 3;
wherein (a) is transmission electron microscope picture of the metal needle point and the metal cut end before the preparation
(b) (c) transmission electron microscope picture of atomic force microscope metal probe appearance and growth process after voltage is applied
(d) The prepared atomic force microscope metal probe picture is obtained;
FIG. 5 is a schematic diagram of the process of preparing the metal probe of the atomic force microscope in example 1, in which the metal tip 1 and the metal open end 2 are respectively connected to the negative electrode and the positive electrode of the power supply 3;
(a) is a schematic view of the metal tip and the metal cut end before the preparation is started.
(b) Is a schematic diagram of the appearance and growth process of the atomic force microscope metal probe after the voltage is applied.
(c) Is a schematic diagram of the process of moving the movable end and separating the two ends.
(d) The preparation of the atomic force microscope metal probe is completed after repeating the operations (b) and (c) for a plurality of times.
FIG. 6 is a schematic diagram of the process of preparing the metal probe of the atomic force microscope in example 1, in which the metal tip 1 and the metal open end 2 are respectively connected to the positive electrode and the negative electrode of the power supply 3;
(a) is a schematic view of the metal tip and the metal cut end before the preparation is started.
(b) Is a schematic diagram of the appearance and growth process of the atomic force microscope metal probe after the voltage is applied.
(c) Is a schematic diagram of the process of moving the movable end and separating the two ends.
(d) The preparation of the atomic force microscope metal probe is completed after repeating the operations (b) and (c) for a plurality of times.
In the figure: 1. a metal needle tip; 2. a metal roughness end; 3. a power source; 4. a metal wire; 5. a movable end; 6. a fixed end; 7. an atomic force microscope metal probe; 8. a metal atom.
Detailed Description
The present invention will be described in further detail below with reference to the accompanying drawings, but the present invention is not limited to the following embodiments.
As shown in fig. 1, the apparatus used for preparation comprises an electrochemical corrosion system, a transmission electron microscope and an electro-mechanical single-inclined sample rod, wherein the transmission electron microscope is used for observing the relative position and movement condition of a metal tip 1 and a metal fracture end 2 and the growth preparation process of a metal probe of an atomic force microscope; the electrochemical corrosion system is used for processing the metal wire to obtain the preparation of the metal needle tip 1.
The electro-mechanical single-inclination sample rod comprises two parts, namely a movable end and a fixed end, wherein the movable end 5 and the fixed end 6 are oppositely arranged and are not in contact with each other, and a metal needle point 1 and a metal cut-off end 2 are respectively fixed on the movable end 5 and the fixed end 6; the metal needle tip 1 and the metal cut-off end 2 are respectively connected with the anode and the cathode of a power supply 3. In the experiment, the movable end is driven to realize accurate control in the up-down direction, the left-right direction, the front-back direction and the three-dimensional direction and apply voltage. In addition, a constant bias voltage may be applied across the sample at the same time.
The preparation process comprises the following steps:
1) preparing a metal cut end 2 by adopting a physical shearing method, specifically, flattening the tail end of a metal wire 4 with the diameter of about 0.25mm and then shearing the metal wire to be used as the metal cut end 2, wherein the root part of the metal cut end 2 is fixed at a fixed end, and the flattened and sheared end part of the metal cut end 2 faces a metal needle point 1;
2) the tail end of the metal wire 4 is treated by adopting an electrochemical corrosion system to carry out electrochemical corrosion, a metal needle point 1 with a sharp tail end is prepared, the diameter of the metal needle point 1 is about 50 nanometers to 200 nanometers, the root of the metal needle point 1 is fixed at a movable end, and the sharp tip at the tail end of the metal needle point 1 faces to a metal cut-off end 2;
3) placing the electro-mechanical single-inclined sample rod into a transmission electron microscope sample cavity, and enabling the metal needle point 1 and the metal cut end 2 to be horizontally aligned and close to each other in the transmission electron microscope sample cavity;
placing the electro-mechanical single-inclination sample rod into a transmission electron microscope, and driving by utilizing piezoelectric ceramics to enable the metal needle point 1 to be horizontally aligned and close to the metal fracture end 2;
4) preparing an atomic force microscope metal probe: applying a certain amount of voltage to two ends of the electricity-mechanics single-inclination sample rod, connecting the metal needle point 1 and the metal cut end 2 with the anode and the cathode of a power supply 3, moving the movable end of the electricity-mechanics single-inclination sample rod under the observation of a transmission electron microscope, moving the movable end of the metal needle point 1 to enable the gap between the metal needle point 1 and the metal cut end 2 to be close to about 2nm, connecting the close parts of the two ends with each other under the action of electromigration to form a single-crystal metal nanowire, then slowly moving the movable end at a constant speed backwards, and finally separating the two ends to obtain a single superfine atomic force microscope metal probe 7 with a certain length;
5) and (4) repeating the step 4) repeatedly to enable the metal probe of the atomic force microscope to grow stably along the axial direction, and regulating and controlling for many times to obtain the metal probe of the atomic force microscope with ideal length and appearance, namely the metal probe 7 of the atomic force microscope with small diameter and large length-diameter ratio.
As shown in fig. 3, the growth direction of the metal probe 7 of the atomic force microscope is controlled by adjusting the polarity of the power supply 3 connected to the metal tip 1 and the metal fracture end 2, and the growth of the metal probe of the atomic force microscope at the metal tip or the metal fracture end can be controlled by changing the voltage direction.
As shown in fig. 5, the metal tip 1 and the metal open end 2 are respectively connected to the negative electrode and the positive electrode of the power supply 3, the metal probe of the atomic force microscope vertically grows from the surface of the metal tip 1 to the direction of the metal open end 2, and the metal atom 8 is left.
As shown in fig. 6, the metal tip 1 and the metal open end 2 are respectively connected to the positive electrode and the negative electrode of the power supply 3, the atomic force microscope metal probe vertically grows from the surface of the metal open end 2 to the direction of the metal tip 1, and the metal atom 8 faces the right.
The length of the metal probe of the atomic force microscope is determined by the voltage, the moving speed and the close repetition times of the steps.
The diameter of the metal probe of the atomic force microscope is determined by the voltage, the shape of the metal tip 1 and the metal cut-off end 2 and the contact area.
The length of the metal probe of the atomic force microscope is increased continuously in the preparation process, but the diameter of the metal probe of the atomic force microscope is not changed obviously.
Example 1
As shown in fig. 3 and 5.
(1) Preparation of metal fracture end 2 by physical shearing
After a tungsten metal wire with the diameter of 0.25mm is subjected to ultrasonic treatment in an ethanol solution for 10min, the tungsten metal wire is flattened by a vice and is cut off by a pair of scissors, at the moment, a large number of small bulges with nanometer sizes are formed on the section of the front end of the metal wire to form a rough surface with nanometer levels, namely a metal cut-off end 2, and a large number of small bulges with nanometer sizes are formed on the front end, and the shapes and the orientations of the small bulges are different. The root of the metal cut end 2 is fixed at the fixed end, and the flattened and sheared end of the metal cut end 2 faces the movable end.
(2) Electrochemical corrosion tungsten wire
The specific implementation adopts a tungsten wire, and ultrasonic cleaning is carried out in an ethanol solution before use to remove surface dirt. Preparing 1mol/L sodium hydroxide solution, combining an electrochemical corrosion system, applying a certain amount of voltage to carry out corrosion to obtain a tungsten metal needle tip 1 with the front end diameter of about 50nm to 200nm, and quickly cutting off the power supply after the corrosion is finished. The root of the metal needle point 1 is fixed at the movable end, and the sharp part of the metal needle point 1 faces the fixed end.
(3) The movable end is close to the fixed end in the transmission electron microscope
Through transmission electron microscope direct observation, the screening obtains the protruding most advanced that satisfies the demands (the appearance is good and the diameter is little, make things convenient for metal needle point rather than the contact, thickness will be little, conveniently calibrate the height and obtain good image), the portable end of constantly adjusting metal needle point 1 moves in upper and lower direction, make metal needle point 1 unanimous with metal cut end 2 at transmission electron microscope sample intracavity level, be in the coplanar each other, the displacement of portable metal needle point 1 in the front and back left and right sides direction is controlled again, as figure 3(a), make metal needle point 1 and metal cut end 2 be close to each other.
(4) A constant bias of 600-. 1V voltage is applied to two ends through the power supply 3, the metal needle point 1 is connected with the negative electrode of the power supply 3, and the metal cut-off end 2 is connected with the positive electrode of the power supply 3. The two end parts are connected with each other under the action of electromigration to form a single crystal metal nanowire.
And moving the movable end of the electro-mechanical single-inclined sample rod under the observation of a transmission electron microscope, and moving the movable end of the metal needle point 1 to enable the gap between the metal needle point 1 and the metal fracture end 2 to be close to about 2 nm. The two ends are connected with each other under the action of electromigration, as shown in fig. 3(b), a single crystal metal nanowire is formed, and the single crystal metal nanowire grows from the surface of the metal needle tip 1 to the direction of the metal fracture end 2. The diameter can not be enlarged during growth, and is only related to the appearance of the two ends at the beginning, the contact area and the voltage.
(5) And slowly moving the movable end of the metal needle tip 1 backwards at a constant speed to separate the two ends to obtain the superfine atomic force microscope metal probe with a certain length.
And slowly moving the movable end of the metal needle tip 1 at a constant speed to enable the movable end to move in a direction far away from the metal cut-off end 2, wherein the moving speed is not too high, so that the two ends are separated and are not contacted any more, and the atomic force microscope metal probe can be separated from the growing non-root end to obtain the superfine atomic force microscope metal probe with a certain length. As can be seen from FIG. 3(c), the atomic force microscope metal probe had a diameter of about 5nm and was very small, which was difficult to obtain by the conventional preparation method.
(6) Repeating the steps (3) to (5) to continuously extend the metal probe of the atomic force microscope
And (5) continuously repeating the steps (3) to (5) to ensure that the metal needle tip 1 is continuously contacted with the metal fracture end 2, the atomic force microscope metal probe stably grows along the axial direction under the action of voltage, the atomic force microscope metal probe with ideal length and appearance is obtained through secondary regulation, and the preparation is finished after the target length is confirmed through transmission electron microscope imaging, as shown in fig. 3(d), so that the atomic force microscope metal probe meeting the requirements is obtained.
Example 2
The difference from the embodiment 1 is that the growth direction is different, the metal needle point 1 is connected with the negative pole of the power supply 3, the metal cut-off end 2 is connected with the positive pole of the power supply 3, and the rest is the same as the embodiment 1. The process is schematically illustrated in fig. 4 and 6, with metal atoms 8 to the right.
Claims (5)
1. A method for preparing a superfine atomic force microscope metal probe is characterized by comprising the following steps: the method comprises the steps that an electro-mechanical single-inclination sample rod is adopted, the electro-mechanical single-inclination sample rod comprises two parts, namely a movable end (5) and a fixed end (6), the movable end (5) and the fixed end (6) are arranged in opposite directions and are not in contact with each other, and a metal needle point (1) and a metal fracture end (2) are respectively loaded on the movable end (5) and the fixed end (6); then the following steps are adopted for processing:
1) preparing the metal fracture end (2) by adopting a physical shearing method, specifically, flattening the tail end of a metal wire (4) and then shearing the metal wire to be used as the metal fracture end (2), wherein the metal fracture end (2) is fixed on a fixed end (6);
2) carrying out electrochemical corrosion treatment on the tail end of the metal wire (4) to prepare a metal needle point (1) with a sharp tail end, wherein the diameter of the metal needle point (1) is in the range of 50 nanometers to 200 nanometers, the root of the metal needle point (1) is fixed at a movable end (5), and the tip of the metal needle point (1) faces towards a metal fracture end (2);
3) placing the electro-mechanical single-inclined sample rod into a transmission electron microscope, and enabling the metal needle point (1) to be horizontally aligned and close to the metal cut end (2) in a transmission electron microscope sample cavity;
4) preparing an atomic force microscope metal probe: applying 600-1000mV constant bias voltage to two ends of the electricity-mechanics single-inclination sample rod, moving the movable end (5) of the electricity-mechanics single-inclination sample rod under the observation of a transmission electron microscope, moving the movable end (5) of the metal needle point (1) to enable the gap between the metal needle point (1) and the metal cut-off end (2) to be close to 2nm, and connecting the two close parts under the action of electromigration to form a single-crystal metal nanowire; then moving the movable end (5) of the metal needle tip (1) at a constant speed in the direction away from the fixed end (6) to separate the two ends to obtain a single superfine atomic force microscope metal probe (7);
5) repeating the step 4) repeatedly, wherein the atomic force microscope metal probe (7) stably grows along the axial direction, and the final atomic force microscope metal probe (7) with ideal length and appearance is obtained through multiple regulation and control;
the growth direction of the atomic force microscope metal probe is controlled by adjusting the polarity of a power supply (3) connected with the metal tip (1) and the metal cut-off end (2).
2. The method for preparing the metal probe of the ultra-fine atomic force microscope according to claim 1, wherein the method comprises the following steps: the diameter of the atomic force microscope metal probe is less than 5 nm.
3. The method for preparing the metal probe of the ultra-fine atomic force microscope according to claim 1, wherein the method comprises the following steps: the metal needle point (1) and the metal fracture end (2) are made of homogeneous metal materials, including tungsten, gold or molybdenum metal materials.
4. The device for preparing the metal probe of the controllable atomic force microscope, which is applied to the method of claim 1, is characterized in that: the device comprises an electrochemical corrosion system, a transmission electron microscope and an electro-mechanical single-inclination sample rod, wherein the transmission electron microscope is used for recording and observing the probe growth preparation condition between a metal needle point (1) and a metal cut end (2) of the electro-mechanical single-inclination sample rod and the relative position and movement condition of the metal needle point (1) and the metal cut end (2); the electrochemical corrosion system is used for processing the metal wire to obtain the preparation of the metal needle point (1);
the metal fracture end (2) is prepared by a physical shearing method, and specifically, the tail end of the metal wire (4) is flattened and then sheared to serve as the metal fracture end (2).
5. The apparatus for preparing the metal probe of the controllable atomic force microscope according to claim 4, wherein: the electro-mechanical single-inclination sample rod comprises two parts, namely a movable end (5) and a fixed end (6), wherein the movable end (5) and the fixed end (6) are oppositely arranged and are not in contact with each other, and a metal needle point (1) and a metal cut-off end (2) are respectively fixed on the movable end (5) and the fixed end (6); the metal needle point (1) and the metal cut-off end (2) are respectively connected with the anode and the cathode of the power supply (3).
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